US11782007B2 - CO2 sensor based on carbon nanotube-functional polymer composite films - Google Patents
CO2 sensor based on carbon nanotube-functional polymer composite films Download PDFInfo
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Definitions
- the present disclosure relates to a novel composite film configured for CO 2 sensing, and the method of making and using the novel composite film.
- Carbon dioxide (CO 2 ) gas levels are commonly monitored within the context of building heating, ventilation, and air conditioning (HVAC) systems as one measure of indoor air quality. While reliable CO 2 sensing is valuable in this and several other laboratory and industrial applications, few commercial CO 2 sensors demonstrate long term reliability in conjunction with low cost and low power consumption. The state-of-the-art application of commercial CO 2 sensors is perhaps best defined by works such as Weekly, et al., which highlights the clear, measurable relationship between CO 2 concentrations in indoor spaces and occupancy through the use of off-the-shelf hardware. See K. Weekly, et al., “Modeling and estimation of the humans' effect on the CO 2 dynamics inside a conference room,” IEEE Transactions on Control Systems Technology , vol. 23, no. 5, pp. 1770-1781, 2015.
- NDIR nondis-persive infrared
- the present disclosure relates to a novel composite film configured for CO 2 sensing, and the method of making and using the novel composite film.
- the present disclosure provides a composite film configured for CO 2 sensing, wherein the composite film comprises a carbon nanotube film and a CO 2 absorbing layer deposited on the carbon nanotube film, wherein the CO 2 absorbing layer comprises a mixture of a branched polyethylenimine, a polyethylene glycol, and poly[1-(4-vinylbenzyl)-3-methylimidazolium tetrafluoroborate] (PVBMIBF4) of formula I:
- n ranges from 10-300.
- FIG. 1 illustrates synthesis of the imidazolium-based PIL (poly(ionic liquid)), PVBMIBF4.
- FIG. 2 illustrates (a) free-floating CNT film generated after casting a dispersion of the CNTs from a concentrated solution.
- the CNT film floating on water is highlighted by the red box.
- the devices with the CNT thin films laminated on them are highlighted by the blue box.
- a separate set of bare electrodes are available but are intentionally not covered with CNTs for visual demonstration purposes.
- FIG. 3 illustrates sensing chamber with six chemiresistive sensors.
- FIG. 4 illustrates measured change in sample resistance to (a) 8,000-20,000 ppm (b) 500 ppm, and (c) 50 ppm CO 2 pulses with a background of 100 ppm CO 2 in N 2 with 40% relative humidity at room temperature.
- the term “about” can allow for a degree of variability in a value or range, for example, within 10%, within 5%, or within 1% of a stated value or of a stated limit of a range.
- the term “substantially” can allow for a degree of variability in a value or range, for example, within 90%, within 95%, or within 99% of a stated value or of a stated limit of a range.
- This disclosure provides another class of sensor, chemiresistive sensors, which have significant promise for low-cost and low-power sensing.
- PEI polyethylenimine
- PEG polyethylene glycol
- ionic liquids have been shown to absorb significant quantities of CO 2 , due to the affinity of CO 2 towards many of the ionic moieties contained within, and thus provide potential utility for increasing the CO 2 uptake of chemiresistive sensors.
- the present disclosure provides a composite film configured for CO 2 sensing, wherein the composite film comprises a carbon nanotube film and a CO 2 absorbing layer deposited on the carbon nanotube film, wherein the CO 2 absorbing layer comprises a mixture of a branched polyethylenimine, a polyethylene glycol, and poly[1-(4-vinylbenzyl)-3-methylimidazolium tetrafluoroborate] (PVBMIBF4) of formula I:
- n ranges from 10-300
- the thickness of said carbon nanotube film is about 10-500 nm, 10-400 nm, 10-300 nm, 10-200 nm, or 10-100 nm.
- the thickness of said CO 2 absorbing layer is 100-1000 nm, 100-900 nm, 100-800 nm, 100-700 nm, 100-600 nm, 100-500 nm. In one aspect, the thickness of said carbon nanotube film is about 100 nm, the thickness of said CO 2 absorbing layer is about 500 nm.
- carbon nanotube film configured for CO 2 sensing, wherein said carbon nanotube film comprises chlorosulfonic acid.
- said branched polyethylenimine has a molar molecular weight of about 1.0-20, 1.0-10, 5-20, 5-10 kg/mol
- said branched polyethylene glycol has a molar molecular weight of about 0.5 kg/mol to 50, 0.5 kg/mol to 40, 0.5 kg/mol to 30 kg/mol.
- the composite film configured for CO 2 sensing wherein said polyethylene glycol has a weight percentage of 40-60% of the total weight of the CO 2 absorbing layer.
- said poly[1-(4-vinylbenzyl)-3-methylimidazolium tetrafluoroborate] has a weight percentage of about 1-10, 1-5, 1-3% of the total weight of the CO 2 absorbing layer.
- said poly[1-(4-vinylbenzyl)-3-methylimidazolium tetrafluoroborate] has a weight percentage of about 1-3% of the total weight of the CO 2 absorbing layer.
- Poly(4-vinylbenzyltrimethylammonium tetrafluoroborate) (PVBMIBF 4 ) was synthesized according to a previous report [See J. Tang, H. Tang, W. Sun, M. Radosz, and Y. Shen, “Poly(ionic liquid)s as new materials for CO 2 absorption,” Journal of Polymer Science Part A: Polymer Chemistry , vol. 43, no. 22, pp. 5477-5489, 2005].
- the reaction scheme is shown in FIG. 1 .
- PEI a highly branched polymer with a rich amount of secondary and tertiary amino groups along the polymer backbone, n-dopes the carbon nanotubes with its electron negative lone pairs.
- the amino groups readily react to form electron deficient ammonium cations, and the n-doping effect is hence weakened, which leads to the change in the carrier concentration within the CNTs. Because this reaction is facilitated by water, PEG is used as a vapor absorbing material, which holds water molecules in this layer.
- the testing chamber as seen in FIG. 3 , was a 114 mm diameter and 20 mm tall cylindrical chamber.
- the walls of the chamber were aluminum.
- the base was a fiberglass printed circuit board (PCB) with the sensors integrated therein and the top was a glass window for observation.
- the 9.5 mm diameter air inlet was located on the aluminum wall. and the 9.5 mm diameter air outlet was fixed to the PCB base.
- the chamber was supplied with gas via an inline flow distribution system with two gas sources: pure nitrogen and a mixture of 1% carbon dioxide and 99% nitrogen.
- the gas sources were connected to three mass flow controllers (MFC) in parallel.
- MFC mass flow controllers
- the nitrogen carrier gas was controlled through two 50 ccm rated MFCs (MKS Instruments 1179C) while the carbon dioxide and nitrogen mixed gas was controlled through a 10 ccm rated MFC (Unit Instruments UFC-1661, 10 ccm). These inlets were connected to a manifold, the output of which was connected directly to the chamber inlet.
- the PCB substrate was secured and the chamber was sealed.
- the chamber was flushed with pure nitrogen at 500 ccm to create an inert environment as a baseline reference. Carbon dioxide was then introduced to the chamber at prescribed concentrations, alternated with nitrogen every 40 min, while maintaining the overall volumetric flow rate constant at 500 ccm for each concentration change.
- the resistances of the electrode pairs were measured using benchtop digital multimeters (Keysight 34401A) over time (sampling rate of 0.5 Hz) and the MFCs were controlled via a custom breakout board connected to an Agilent Technologies U2781A USB module DAQ chassis containing U2541A modular USB data acquisition modules, which provided analog input and output. The control of the MFCs and sampling from the multimeters was facilitated with a National Instruments LabVIEW virtual instrument program.
- a discernible response signal was first obtained by measuring the resistance across each sensor with a benchtop digital multimeter. The relative response shift was then calculated as:
- FIG. 4 shows the sensor response to high concentrations of CO 2 in ranges relevant to industrial applications and human respiration monitoring.
- FIG. 4 ( b ) and FIG. 4 ( c ) show sensor response in ranges relevant to indoor air quality monitoring and occupancy monitoring.
- NDIR-type sensors are the most common commercially available CO 2 sensors given their accuracy at a relatively low cost. An accuracy of ⁇ 20 ppm was established for some commercially available NDIR CO 2 sensors in the sub 50,000 ppm range [See S. K. Pandey and K.-H. Kim, “The relative performance of NDIR-based sensors in the near real-time analysis of CO 2 in air,” Sensors , vol. 7, no. 9, pp. 1683-1696, 2007]. In another analysis of the performance of commercial NDIR CO 2 sensors [See T. Yasuda, S. Yonemura, and A. Tani, “Comparison of the characteristics of small commercial NDIR CO 2 sensor models and development of a portable CO 2 measurement device,” Sensors, vol. 12, no.
- NDIR sensors with an accuracy of ⁇ 30 ppm were evaluated. These sensors were shown to be able to respond to small changes (less than 100 ppm) in CO 2 concentration around room limits (e.g., under 1000 ppm).
- the chemiresistive sensors tested here exhibit clear response deviations in the presence of 50 ppm of CO 2 on a 100 ppm background, which is comparable to their commercial NDIR counterparts. Accordingly, the examined device shows promise as a CO 2 sensor that can sense the gas at a lower cost, and with lower power, than traditional detection methods.
- chemiresistive devices comprised of a PEI-PEG-PIL and CNT combination, successfully sensed changes in CO 2 concentration. It was found that the change in resistance from an initial value was a monotonic function of the CO 2 concentration in the surrounding environment. Given the relatively low cost and their potential for low power consumption, these chemiresistive sensors serve as an attractive alternative to current commercially available CO 2 sensors.
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Abstract
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- wherein n ranges from 10-300.
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WO2018216017A1 (en) | 2017-05-24 | 2018-11-29 | Technion Research And Development Foundation Ltd. | Carbon dioxide sensors comprising poly(ionic liquid) |
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US20090266230A1 (en) * | 2004-08-05 | 2009-10-29 | Maciej Radosz | Poly(ionic liquid)s as new materials for co2 separation and other applications |
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KR20170044529A (en) * | 2015-10-15 | 2017-04-25 | 엘지전자 주식회사 | Graphene for sensing carbon dioxide and fabrication method thereof |
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